JP5945914B2 - Cleaning agent for removing flux residue - Google Patents
Cleaning agent for removing flux residue Download PDFInfo
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- JP5945914B2 JP5945914B2 JP2012044137A JP2012044137A JP5945914B2 JP 5945914 B2 JP5945914 B2 JP 5945914B2 JP 2012044137 A JP2012044137 A JP 2012044137A JP 2012044137 A JP2012044137 A JP 2012044137A JP 5945914 B2 JP5945914 B2 JP 5945914B2
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本発明は、保管時には均質な溶液である一方、使用時には白濁状態となり、フラックス残渣を好適に除去できる洗浄剤に関する。 The present invention relates to a cleaning agent that is a homogeneous solution during storage, becomes cloudy during use, and can suitably remove flux residues.
フラックス残渣とは、ICやコンデンサ、抵抗器等の電子部品をプリント基板等にハンダ付した際、ハンダ接合部付近に残留するフラックス成分をいう。フラックスとしては一般にロジン類をベース材としたもの(以下、ロジン系フラックスという)が使用されており、電極に直接塗布する場合もあれば、ハンダ合金粉末と混合しハンダペーストとして使用される場合もあり、表面実装基板の製造においては後者の態様が主流である。 The flux residue refers to a flux component that remains in the vicinity of the solder joint when an electronic component such as an IC, a capacitor, or a resistor is soldered to a printed circuit board or the like. As a flux, a rosin base material (hereinafter referred to as a rosin flux) is generally used. It may be applied directly to the electrode, or it may be mixed with solder alloy powder and used as a solder paste. In the manufacture of surface mount substrates, the latter mode is mainstream.
ハンダペーストによる表面実装のプロセスは様々であるが、一例を挙げると、プリント基板の電極上にハンダペーストがスクリーン印刷やディスペンサー等によって供給され、その上に電子部品を載置し、当該基板をハンダ金属の融点以上に加熱することによって、電子部品と電極が接合される。 There are various surface mounting processes using solder paste. For example, solder paste is supplied onto electrodes of a printed circuit board by screen printing or a dispenser, and electronic components are placed on the solder paste. By heating the metal to a melting point or higher, the electronic component and the electrode are joined.
前記のようにハンダ付は高温で行われるため、ハンダペーストからロジン系フラックスが飛散し、電極周囲に残渣として付着することがある。残渣は少量であれば格別問題ないが、多量であると表面実装基板の検品作業や信頼性に悪影響が及ぶ。一方、ハンダ接合部はフラックス残渣膜により不可避的に覆われるが、残渣中の酸成分(樹脂酸、活性剤等)による腐食が進行したり、残渣膜表面の微細なクラックにおいて所謂マイグレーション現象による悪影響を受けたりする。 As described above, since soldering is performed at a high temperature, the rosin-based flux may be scattered from the solder paste and adhere as a residue around the electrode. If the amount of residue is small, there is no particular problem, but if the amount is large, the inspection work and reliability of the surface mount substrate will be adversely affected. On the other hand, the solder joint is inevitably covered with the flux residue film, but corrosion due to acid components (resin acid, activator, etc.) in the residue proceeds, or the adverse effect due to the so-called migration phenomenon in the minute cracks on the residue film surface. Or receive.
それゆえ、フラックス残渣は通常、各種洗浄剤で除去する必要があり、斯界では従来、ロジン系フラックスに適した洗浄剤として様々な製品が提案されてきた(例えば特許文献1〜3を参照。)。本出願人も例えば、ポリオキシアルキレングリコールエーテルやポリオキシアルキレングリコールエステル等のグリコール系溶剤からなる洗浄剤を種々提案している(例えば特許文献4〜7を参照。)。 Therefore, the flux residue usually needs to be removed with various cleaning agents, and various products have been proposed in the art as cleaning agents suitable for rosin flux (see, for example, Patent Documents 1 to 3). . The present applicant has also proposed various cleaning agents composed of glycol solvents such as polyoxyalkylene glycol ethers and polyoxyalkylene glycol esters (see, for example, Patent Documents 4 to 7).
ところで、これら洗浄剤は一般的に、洗浄効率を高めるべく50〜60℃程度に加温された状態で使用されるが、粘度を下げて取り扱いをよくしたり、VOC排出を抑えたりするために、洗浄現場では洗浄剤を予め水で希釈することがある。しかし、当然のことではあるが、水の配合量を多くすればするほど洗浄成分である有機溶剤の比率が低下するため、フラックス残渣を十分に除去できなくなる。 By the way, these cleaning agents are generally used in a state of being heated to about 50 to 60 ° C. in order to increase the cleaning efficiency. However, in order to reduce the viscosity to improve the handling or to suppress the VOC emission. In the cleaning site, the cleaning agent may be diluted with water in advance. However, as a matter of course, the larger the amount of water added, the lower the ratio of the organic solvent that is a cleaning component, so that the flux residue cannot be removed sufficiently.
こうした問題を解消するべく、例えば特許文献8において、SP(溶解度パラメータ)値が異なる3種の有機溶剤を組み合わせた洗浄剤が提案されている。このものは、水を配合する前は均一な溶液であるが、使用前に比較的多量の水を配合し撹拌することによって白濁し、その状態においてフラックス残渣を好適に除去するとされている。しかし、使用直前に水を都度配合しなければならないため、作業性の点で難がある。また、この洗浄剤は水を加えた後に長時間放置すると有機溶剤と水の二層に分離するため、洗浄剤が余った場合、次に使用する際に再度撹拌しなければならないという点でも不便である。 In order to solve such a problem, for example, Patent Document 8 proposes a cleaning agent in which three kinds of organic solvents having different SP (solubility parameter) values are combined. This is a uniform solution before blending water, but becomes cloudy by blending and stirring a relatively large amount of water before use, and the flux residue is suitably removed in that state. However, since water must be added each time immediately before use, there is a difficulty in workability. Also, since this cleaning agent is separated into two layers when it is left for a long time after adding water, it is inconvenient in that if the cleaning agent is left, it must be stirred again when it is used next time. It is.
本発明は、常温では均質な水溶液であるが、使用時(加温時)には白濁状態となってフラックス残渣を好適に除去できる、新規な洗浄剤を提供することを課題とする。 An object of the present invention is to provide a novel cleaning agent that is a homogeneous aqueous solution at normal temperature, but becomes cloudy at the time of use (warming) and can suitably remove a flux residue.
本発明者は鋭意検討した結果、所定のノニオン系化合物からなる有機溶剤に水を比較的多量に含ませた水溶液が前記課題を達成する洗浄剤として有用であることを見出した。 As a result of intensive studies, the present inventor has found that an aqueous solution in which a relatively large amount of water is contained in an organic solvent composed of a predetermined nonionic compound is useful as a cleaning agent for achieving the above-described problem.
即ち本発明は、プロピルプロピレングリコール、プロピルプロピレンジグリコール及びブチルプロピレングリコールからなる群より選ばれる少なくとも一種の分岐状ノニオン化合物(1)と、ブチルジグリコール及びヘキシルジグリコールからなる群より選ばれる少なくとも一種の直鎖状ノニオン化合物(2)とからなる有機溶剤(A)20〜40重量%、ならびに水(B)60〜80重量%を含有し、かつ、前記式(1)の分岐状ノニオン系化合物と式(2)の直鎖状ノニオン系化合物との重量比((1)/(2))が0.5/3〜3/0.3であり、かつ、曇点が20〜90℃である水溶液を用いてなる、フラックス残渣除去用洗浄剤;ブチルジグリコール及びヘキシルジグリコールからなる群より選ばれる少なくとも一種の直鎖状ノニオン化合物(2)からなる有機溶剤(A)20〜40重量%、ならびに水(B)60〜80重量%を含有し、かつ、曇点が20〜90℃である水溶液を用いてなる、フラックス残渣除去用洗浄剤;当該洗浄剤をその曇点以上の温度でフラックス残渣が付着した被洗浄物に接触させることを特徴とする、物品の洗浄方法、に関する。 That is, the present invention provides at least one branched nonionic compound (1) selected from the group consisting of propylpropylene glycol, propylpropylene diglycol and butylpropylene glycol, and at least one selected from the group consisting of butyl diglycol and hexyl diglycol. A branched nonionic compound of the formula (1) containing 20 to 40% by weight of an organic solvent (A) and 60 to 80% by weight of water (B) comprising the linear nonionic compound (2) And the weight ratio ((1) / (2)) of the linear nonionic compound of formula (2) is 0.5 / 3 to 3 / 0.3, and the cloud point is 20 to 90 ° C. It made using certain aqueous detergent flux residue removal, at least one linear Noni selected from the group consisting of butyl diglycol and hexyl diglycol A flux comprising an organic solvent (A) comprising 20 to 40% by weight of an organic compound (2) and 60 to 80% by weight of water (B) and having a cloud point of 20 to 90 ° C. The present invention relates to a method for cleaning an article, characterized by bringing the cleaning agent into contact with an object to be cleaned to which a flux residue has adhered at a temperature equal to or higher than the cloud point.
本発明の洗浄剤は、前記したように、常温では均質な水溶液であるが、その曇点以上に加温することによって二層に分離し、さらにその状態で撹拌することにより白濁する。そして、この白濁状態の洗浄剤により、フラックス残渣を好適に除去することが可能になる。また、本発明の洗浄剤に添加剤としてアミノアルコール類を配合した場合には、洗浄後に析出物が発生し難くなるため、繰り返し使用に適するようになる。また、常温では均質であることより一液の状態で貯蔵できる利点もある。また、揮発性が高いため、後の水リンス工程を設ける必要が特になく、全行程の簡素化を図ることもできる。その他、水の含有量が多いため、VOC排出量も少なく、非危険物として取り扱うことができる。 As described above, the cleaning agent of the present invention is a homogeneous aqueous solution at room temperature, but is separated into two layers by heating above its cloud point, and becomes cloudy when further stirred in that state. And it becomes possible to remove a flux residue suitably by this cleaning agent of a cloudy state. In addition, when an amino alcohol is added as an additive to the cleaning agent of the present invention, precipitates are less likely to be generated after cleaning, so that it is suitable for repeated use. In addition, there is an advantage that it can be stored in one liquid state because it is homogeneous at room temperature. Moreover, since it is highly volatile, it is not particularly necessary to provide a subsequent water rinsing step, and the entire process can be simplified. In addition, since the water content is high, VOC emissions are small and can be handled as non-hazardous materials.
本発明の洗浄剤はプロピルプロピレングリコール、プロピルプロピレンジグリコール及びブチルプロピレングリコールからなる群より選ばれる少なくとも一種の分岐状ノニオン化合物(1)と、ブチルジグリコール及びヘキシルジグリコールからなる群より選ばれる少なくとも一種の直鎖状ノニオン化合物(2)とからなる有機溶剤(A)20〜40重量%、ならびに水(B)60〜80重量%を含有し、かつ、前記式(1)の分岐状ノニオン系化合物と式(2)の直鎖状ノニオン系化合物との重量比((1)/(2))が0.5/3〜3/0.3であり、かつ、曇点が20〜90℃である水溶液を用いたものと、ブチルジグリコール及びヘキシルジグリコールからなる群より選ばれる少なくとも一種の直鎖状ノニオン化合物(2)からなる有機溶剤(A)20〜40重量%、ならびに水(B)60〜80重量%を含有し、かつ、曇点が20〜90℃である水溶液を用いたものとである。 The cleaning agent of the present invention is at least one branched nonionic compound (1) selected from the group consisting of propylpropylene glycol, propylpropylene diglycol and butylpropylene glycol, and at least selected from the group consisting of butyl diglycol and hexyl diglycol. An organic solvent (A) comprising 20 to 40% by weight of a linear nonionic compound (2) and 60 to 80% by weight of water (B), and a branched nonionic system of the formula (1) The weight ratio of the compound to the linear nonionic compound of formula (2) ((1) / (2)) is 0.5 / 3 to 3 / 0.3, and the cloud point is 20 to 90 ° C. and that an aqueous solution is composed of at least one linear nonionic compound (2) is selected from the group consisting of butyl diglycol and hexyl diglycol Machine solvent (A) 20 to 40 wt%, and contain water (B) 60-80 wt%, and is to that cloud point using an aqueous solution is 20 to 90 ° C..
なお、必要に応じ、(A)成分とともに、前記化合物(1)および化合物(2)以外の成分として、ポリオキシアルキレンアルキルエーテル、ポリオキシアルキレンフェノールエーテル、ポリオキシアルキレンアルキルフェノールエーテルや、ポリアルキレングリコールモノエステル、ポリアルキレングリコールジエステル等のポリアルキレングリコールエステル等を併用できる。 Incidentally, if necessary, with the component (A), as a component other than the compound (1) and the compound (2), polyoxyalkylene alkyl ethers, polyoxyalkylene phenols ethers, and polyoxyalkylene alkylphenol ethers, polyalkylene glycol mono Polyalkylene glycol esters such as esters and polyalkylene glycol diesters can be used in combination.
(B)成分としては、イオン交換水、純水、市水等が挙げられる。 (B) As an ingredient, ion exchange water, pure water, city water, etc. are mentioned.
本発明の洗浄剤における(A)成分及び(B)成分の含有量は特に限定されないが、本発明の洗浄剤の常温での透明性、使用時(加温下での撹拌時)での白濁性、及びフラックス残渣の除去性能を考慮して、順に20〜40重量%程度および60〜80重量%程度であり、好ましくは25〜35重量%および65〜75重量%である。 The content of the component (A) and the component (B) in the cleaning agent of the present invention is not particularly limited, but the cleaning agent of the present invention is transparent at room temperature and cloudy at the time of use (at the time of stirring under heating). In consideration of the property and the removal performance of the flux residue, the amount is about 20 to 40% by weight and about 60 to 80% by weight, preferably 25 to 35% by weight and 65 to 75% by weight.
本発明の洗浄剤はその曇点である20〜90℃を境に前記白濁の有無を判断する。ここに曇点とは、JIS K3211で定義される用語であり、本発明においては、洗浄剤を昇温させたときに二層に分離し始める温度をいう。曇点は、好ましくは25〜70℃程度、いっそう好ましくは30〜50℃程度である。 The cleaning agent of the present invention determines the presence or absence of the cloudiness at a clouding point of 20 to 90 ° C. Here, the cloud point is a term defined in JIS K3211, and in the present invention, it refers to a temperature at which the cleaning agent starts to separate into two layers when the temperature is increased. A cloud point becomes like this. Preferably it is about 25-70 degreeC, More preferably, it is about 30-50 degreeC.
(A)成分の物性は格別限定されないが、被洗浄物の乾燥性の点より沸点が通常200℃以下、好ましくは140〜200℃程度、いっそう好ましくは140〜180℃程度のものが好ましい。 Although the physical properties of the component (A) are not particularly limited, those having a boiling point of usually 200 ° C. or less, preferably about 140 to 200 ° C., more preferably about 140 to 180 ° C. are preferable from the viewpoint of the drying property of the object to be cleaned.
本発明に係る水溶液には、被洗浄物の汚染物質を洗浄剤中に安定して溶解または分散させル目的で、各種公知のアミノアルコール(C)(以下、(C)成分という)を含めることができる。具体的には、直鎖状または分岐状のアルキル基(炭素数1〜5程度)を有するアミノアルコールが挙げられ、n−ブチルジエタノールアミン、エチルエタノールアミン、n−ブチルエタノールアミン等を例示できる。また、(C)成分は、フラックス残渣がロジンをベース材とするフラックスによるものであるときに特に有効であり、洗浄後に当該フラックスの成分に由来する析出物が発生し難くなる。また、(C)成分としては、被洗浄物の乾燥性を加味すると、沸点250℃未満のものが、特に沸点150〜200℃程度のものが好ましい。本発明の洗浄剤における(C)成分の含有量は特に限定されないが、本発明に係る水溶液100重量%とした場合に通常0〜5重量%程度、好ましくは0.1〜1重量%となる範囲である。 In the aqueous solution according to the present invention, various known amino alcohols (C) (hereinafter referred to as component (C)) are included for the purpose of stably dissolving or dispersing contaminants in the cleaning object in the cleaning agent. Can do. Specific examples include amino alcohols having a linear or branched alkyl group (having about 1 to 5 carbon atoms), and examples thereof include n-butyldiethanolamine, ethylethanolamine, and n-butylethanolamine. In addition, the component (C) is particularly effective when the flux residue is derived from a rosin-based flux, and precipitates derived from the flux components are less likely to occur after cleaning. In addition, as the component (C), considering the drying property of the object to be cleaned, those having a boiling point of less than 250 ° C., particularly those having a boiling point of about 150 to 200 ° C. are preferable. The content of the component (C) in the cleaning agent of the present invention is not particularly limited, but is usually about 0 to 5% by weight, preferably 0.1 to 1% by weight when the aqueous solution according to the present invention is 100% by weight. It is a range.
本発明の物品の洗浄方法は、本発明の洗浄剤をその曇点以上の温度でフラックス残渣が付着した被洗浄物に接触させることを特徴とする。被洗浄物としては、フラックス残渣、具体的にはロジン系フラックス残渣が付着したものであれば特に限定されない。例えば、ICやコンデンサ、抵抗器等の電子部品を、ロジン系フラックスを含むハンダペーストによってプリント基板に表面実装したものが挙げられる。また、ロジン系フラックスとしては、一般にロジン類をベース材としてものあれば特に限定されず、他に各種活性剤やチキソトロピック剤、添加剤等を含んでいてよい。 The method for cleaning an article of the present invention is characterized in that the cleaning agent of the present invention is brought into contact with an object to be cleaned to which a flux residue adheres at a temperature equal to or higher than the cloud point. The object to be cleaned is not particularly limited as long as a flux residue, specifically, a rosin flux residue adheres thereto. For example, an electronic component such as an IC, a capacitor, or a resistor may be surface-mounted on a printed board with a solder paste containing a rosin flux. The rosin flux is not particularly limited as long as rosin is used as a base material, and may contain various activators, thixotropic agents, additives, and the like.
被洗浄物に本発明の洗浄剤を接触させる手段は特に限定されず、例えば浸漬洗浄やシャワー洗浄、超音波洗浄、液中ジェット洗浄等の各種方法が挙げられる。また、洗浄の際に各種ミキシング手段を併用することにより、白濁状態が達成される。 Means for bringing the cleaning agent of the present invention into contact with an object to be cleaned is not particularly limited, and examples thereof include various methods such as immersion cleaning, shower cleaning, ultrasonic cleaning, and submerged jet cleaning. Moreover, a cloudy state is achieved by using various mixing means together at the time of washing | cleaning.
また、洗浄後の被洗浄物は乾燥工程に付される。乾燥後の水リンス工程は特に必要ないが、設ける場合には、リンス温度を本発明の洗浄剤の曇点以下とすることにより、前記化合物(1)および化合物(2)をリンス水で除去しやすくなる。 Moreover, the to-be-cleaned object after washing | cleaning is attached | subjected to a drying process. The water rinsing step after drying is not particularly necessary, but when provided, the compound (1) and the compound (2) are removed with rinsing water by setting the rinsing temperature below the cloud point of the cleaning agent of the present invention. It becomes easy.
以下、実施例を通じて本発明をより具体的に説明するが、本発明の範囲がそれらによって何ら限定されないことはもとよりである。なお、部は重量基準である。 Hereinafter, the present invention will be described in more detail through examples, but the scope of the present invention is not limited to these examples. Parts are based on weight.
<洗浄剤組成物の調製>
実施例1
(A)成分としてプロピルプロピレングリコール30部、(B)成分として純水70部をビーカーに入れ、よく撹拌することにより洗浄剤組成物を調製した。
<Preparation of cleaning composition>
Example 1
A cleaning composition was prepared by placing 30 parts of propylpropylene glycol as component (A) and 70 parts of pure water as component (B) into a beaker and stirring well.
実施例1〜5、比較例1
各成分を表1に変更した他は実施例1に順じて洗浄剤組成物を調製した。なお、表中の数字は部数を示す。
Examples 1-5, Comparative Example 1
A cleaning composition was prepared in the same manner as in Example 1 except that each component was changed to Table 1. The numbers in the table indicate the number of copies.
<洗浄試験用試験板の作製>
市販の銅板(2.0cm×4.0cm×0.3mm)にリング状の鉛フリーハンダ合金を載せた。次いで、市販のアクリル化ロジン(商品名「KE−604」、荒川化学工業(株)製)とイソプロピルアルコールからなるフラックス溶液(不揮発分80%)をリング内部にスポイドで三滴注入した。次いで当該銅板をホットプレートに載せ、250℃で加熱し、鉛フリーハンダ合金を溶融させたところ、フラックス残渣で覆われたドーム状のハンダ合金が残された。このようにして得られた銅板を洗浄試験基板Aとする。
<Preparation of test plate for cleaning test>
A ring-shaped lead-free solder alloy was placed on a commercially available copper plate (2.0 cm × 4.0 cm × 0.3 mm). Next, three drops of a commercially available acrylated rosin (trade name “KE-604”, manufactured by Arakawa Chemical Industries, Ltd.) and isopropyl alcohol (nonvolatile content 80%) were injected into the ring with a dropper. The copper plate was then placed on a hot plate and heated at 250 ° C. to melt the lead-free solder alloy, leaving a dome-shaped solder alloy covered with the flux residue. The copper plate thus obtained is used as a cleaning test substrate A.
前記フラックス溶液に代えて、荒川化学工業(株)製の鉛フリーハンダフラックス(商品名「A59−26−35」;ベースロジンとしてKE−604、その他各種活性剤含む)とイソプロピルアルコールからなるフラックス溶液(不揮発分80%)を用い、前記同様の方法によりハンダ合金付の銅板を作製した。これを洗浄試験基板Bとする。 Instead of the flux solution, a flux solution made of Arakawa Chemical Industries, Ltd., lead-free solder flux (trade name “A59-26-35”; KE-604 as base rosin and other various active agents) and isopropyl alcohol A copper plate with a solder alloy was prepared by the same method as above using (nonvolatile content 80%). This is designated as a cleaning test substrate B.
<洗浄試験>
実施例1の洗浄剤組成物を100mLのビーカーに入れ、60℃に加温して、スターラーで撹拌し、懸濁状態にした。次いで、その状態の洗浄剤組成物に前記洗浄試験板AとBを浸漬し、フラックス残渣が溶解するまでの時間をそれぞれ測定し、以下の基準で洗浄力を評価した。他の実施例及び比較例の洗浄液組成物についても同様に洗浄力を評価した。
<Cleaning test>
The cleaning composition of Example 1 was put in a 100 mL beaker, heated to 60 ° C., stirred with a stirrer, and suspended. Next, the cleaning test plates A and B were immersed in the cleaning composition in that state, the time until the flux residue was dissolved was measured, and the cleaning power was evaluated according to the following criteria. The cleaning powers of the cleaning liquid compositions of other examples and comparative examples were similarly evaluated.
3分未満・・・◎
3分以上、4分未満・・・○
4分以上、5分未満・・・△
5分以上・・・×
Less than 3 minutes ... ◎
3 minutes or more, less than 4 minutes ... ○
4 minutes or more and less than 5 minutes ... △
5 minutes or more ×
<析出物の確認>
洗浄試験後、撹拌を止め、洗浄液の前記温度を維持した状態でその外観を観察し、析出物の発生の有無を以下の基準で目視判断した。
<Confirmation of precipitate>
After the cleaning test, stirring was stopped, the appearance of the cleaning liquid was maintained while maintaining the temperature, and the presence or absence of precipitates was visually determined based on the following criteria.
析出物無し・・・○
析出物有り・・・×
No precipitate ... ○
There is a deposit ... ×
PFG:プロピルプロピレングリコール
PFDG:プロピルプロピレンジグリコール
BDG:ブチルジグリコール
HeDG:ヘキシルジグリコール
MEM:エチルエタノールアミン
PFG: propyl propylene glycol PFDG: propyl propylene diglycol BDG: butyl diglycol HeDG: hexyl diglycol MEM: ethyl ethanolamine
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